Published:Journal of Chromatographic Science, ISSN 0021-9665 Volume 47, Number 7, August 2009, pp. 523-528

The Determination of Haloacetic Acids in Real World Samples using IC–ESI-MS–MS

Rosanne Slingsby, Charanjit Saini, and Christopher Pohl
Dionex Corp., R&D

This paper presents the determination of nine haloacetic acids (HAAs) in high ionic strength, treated effluent waters using an ion chromatography–electrospray ionization-tandem mass spectrometry (IC–ESI-MS–MS) method with internal standards and discussions of each of the method parameters. Data is also provided for these same samples using USEPA Method 552.2. The sample matrices contain up to 170 mg/L chloride and 243 mg/L sulfate. Matrix ions are separated from the analytes using a high capacity anion exchange analytical column and diverted to a waste stream during each analysis to avoid signal suppression and contamination of the detector. No derivatization, offline matrix elimination, or preconcentration is used. Four isotopically-labeled HAAs are used for quantification, and detection limits are in the range of 400–1000 µg/L with R² of at least 0.997 over two orders of magnitude for all analytes in matrix. A trichloroacetic acid (TCAA) internal standard with the label on the alpha carbon is found to be more stable than the TCAA-1-¹³C. Amounts found using IC–MS–MS are 65–130% of amounts found using Method 552.2 for all analytes in the real world treated effluent waters. Detection limits for all nine analytes in matrix are in the range of 100–700 ng/L.

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